Methanol → Methyl 4-Iodo-3-methylbenzoate

HRID 840487

反応式

HRID 840487 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[I:11])[C:5]([OH:7])=[O:6].S(=O)(=O)(O)O.[CH3:17]O>>[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[I:11])[C:5]([O:7][CH3:17])=[O:6]

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 15173224-Iodo-3-methylbenzoic acid

生成物 1

HCID 231757Methyl 4-Iodo-3-methylbenzoate

実験手順

24.4 g (0.093 mol) of 3-methyl-4-iodobenzoic acid and 250 ml of methanol were introduced into a round-bottomed flask and 2.5 ml of concentrated sulfuric acid were added dropwise. Heating was carried out at reflux for twelve hours, the reaction mixture was evaporated and the residue taken up in ethyl acetate and water. The organic phase was separated by settling, dried over magnesium sulfate and evaporated. The residue was triturated in methanol and filtered. 21.9 g (85%) of the expected methyl ester, with a melting point of 58°-59° C., were recovered.

後処理

  1. temperatureHeating
  2. temperatureat reflux for twelve hours
  3. customthe reaction mixture was evaporated
  4. customThe organic phase was separated
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. customThe residue was triturated in methanol
  8. filtrationfiltered
  9. custom21.9 g (85%) of the expected methyl ester, with a melting point of 58°-59° C., were recovered

出典と根拠

ORDレコード
ord-28e714b4d999404bbb4c92a95d3104a7
出典データセット
uspto-grants-2002_04
特許番号
US06368608B1

関連ノート

読み込み中…